Qualitative and Quantitative Determination of Dapagliflozin Propanediol Monohydrate and Its Related Substances and Degradation Products Using LC-MS and Preparative Chromatography Methods

Dapagliflozin is a novel sodium-glucose cotransporter type 2 inhibitor. This work aims to develop new validated sensitive RP-HPLC coupled with mass detector method for the determination of dapagliflozin, its alpha isomer, and starting material in presence dapagliflozin major degradation products an internal standard (empagliflozin). The separation was achieved on BDS Hypersil column (length 250mm, diameter 4.6 mm 5-μm particle size) at temperature 35℃. Water acetonitrile were used as mobile phase A B by gradient mode flow rate 1 mL/min. wavelength 224nm selected perform detection using photo diode array detector. met requirement International Conference Harmonisation Registration Pharmaceuticals Human Use (ICH) validation. molecular weight impurities estimated positive ESI-MS. Fifteen detected during analysis APIs brand Farxiga ® some generic products. Three fifteen (H, J K) exceeded acceptable limits 0.1%. Those isolated preparative chromatography then characterized elemental analysis, FTIR NMR.